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Hierarchical Ni-Co double transition metal hydroxide nanosheets have been explored as an effective strategy for the design of nonenzymatic glucose sensors. Ni-Co hydroxide nanosheets constructed hollow cubes were successfully synthesized by using Cu2O cubes as templates and subsequently etched by Na2S2O3 to achieve a hollow cubic structure. The molar ratio between Ni and Co was tuned by varying the precursor ratio of NiCl2 and CoCl2. It was observed by transmission electron microscopy (TEM) that the increasing Ni precursor resulted in particle morphology, and the increasing ratio of the Co precursor resulted in more lamellar morphology. The sample with the composition of Ni0.7Co0.3(OH)2 displayed the best performance for glucose sensing with high selectivity (1541 μA mM–1 cm–2), low detection limit (3.42 µM with S/N = 3), and reasonable selectivity. Similar strategies could be applied for the design of other electrode materials with high efficiency for nonenzymatic glucose determination. [ABSTRACT FROM AUTHOR]